CN110404558A - It is a kind of to decompose the NiPt-Ni (OH) for producing hydrogen for hydrazine2/La(OH)3Catalyst and preparation method thereof - Google Patents
It is a kind of to decompose the NiPt-Ni (OH) for producing hydrogen for hydrazine2/La(OH)3Catalyst and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/894—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1052—Nickel or cobalt catalysts
- C01B2203/1058—Nickel catalysts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/12—Feeding the process for making hydrogen or synthesis gas
- C01B2203/1205—Composition of the feed
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention provides a kind of NiPt-Ni (OH) that production hydrogen is decomposed for hydrazine2/La(OH)3Catalyst and preparation method thereof.The catalyst is by W metal, Pt metal, metal hydroxides Ni (OH)2With rare earth element hydroxide La (OH)3Carrier composition, structural formula are NiPt-Ni (OH)2/La(OH)3.The catalyst is first passed through alkaline chemical precipitation and is obtained Ni (OH) using precipitating reduction method2With Pt (OH)2, sodium borohydride reduction is then added and obtains.The catalyst can decompose production hydrogen by quick catalysis hydrazine under conditions of normal temperature and pressure does not add any auxiliary agent, and selectivity up to 95%, conversion frequency is up to 303h‑1.The catalyst preparation is simple, and catalytic activity is high, is a kind of very promising catalyst.
Description
Technical field
The method of the present invention is related to a kind of composite nano-catalyst and preparation method thereof for decomposing for hydrazine and producing hydrogen, belongs to hydrogen storage
Material Field.
Background technique
Hydrogen Energy is free of contamination due to having the characteristics that heats of combustion value and combustion product, it is considered to be a kind of ideal secondary energy
Source.But how safely and efficiently to store hydrogen is still to restrict the bottleneck of the large-scale use of Hydrogen Energy.Chemical hydrogen storage material
Due to hydrogen-storage density with higher, be readily transported and store, be can substitute tradition pressurization or low-temperature liquefaction hydrogen storage it is new
Type hydrogen storage mode.In all chemical hydrogen storage materials, hydrazine hydrate hydrogen content with higher, and can be straight on existing
Use is connect, is a kind of chemical hydrogen storage material of great application prospect.
Hydrazine hydrate (N2H4·H2O), physicochemical properties are stablized at room temperature, are readily transported and store, hydrogen storage content is
8.0wt.%, the requirement index (5.5wt%) for the hydrogen storage materials in 2017 that remote super U.S. Department of Energy is formulated, has good reality
Application prospect.In the presence of having suitable catalyst, the decomposition of hydrazine hydrate just can be carried out under mild conditions.Theoretically 1 mole
Hydrazine hydrate decompose and can produce 2 moles of hydrogen and nitrogen (reaction 1).But the decomposition of hydrazine hydrate is often accompanied by generation ammonia
The generation (reaction 2) of the side reaction of gas, will be greatly reduced the efficiency that hydrazine hydrate produces hydrogen.Therefore, the key that hydrazine hydrate produces hydrogen is
Prepare high activity, highly selective catalyst.
N2H4(l)→N2(g)+2H2(g) (1)
3N2H4(l)→4NH3(g)+N2(g) (2)
The method for usually improving the hydrogen selective that hydrazine hydrate decomposes, which has, increases reaction temperature and addition alkali as auxiliary agent
(J.Am. Chem.Soc.2010,49,6148；Eur.J.Inor.Chem.2011,2011,2232).However, increasing temperature meaning
Taste the increase of production cost and energy consumption, and the introducing of sodium hydroxide can corrode equipment, propose more to equipment and operation
High requirement.Therefore, how under conditions of room temperature and alkali-free efficient catalytic hydrazine hydrate produces hydrogen, be that realize that hydrazine hydrate produces hydrogen real
The key of border application.It is taken off currently, the catalyst that there are reports can be realized Compounds with Hydrazine Hydrate Catalyzed highly selective at room temperature
Hydrogen (Angew. Chem., Int.Ed.2012,51,1；J.Mater.Chem.A 2016,4,6595), but these catalyst
Catalytic activity is still very low, is unable to satisfy the needs of actual production.Therefore, one kind is prepared under the conditions of room temperature alkali-free, it can be high
The catalyst that the highly selective Compounds with Hydrazine Hydrate Catalyzed of activity produces hydrogen has very important theoretical and practical significance.
Summary of the invention
The purpose of the present invention is to provide a kind of composite nano-catalysts and preparation method thereof, which can
To produce hydrogen for liquid-phase catalysis hydrazine.Herein, the composite nano-catalyst is also known as NiPt-Ni (OH)2/La(OH)3It urges
Agent.
NiPt-Ni (OH) of the present invention2/La(OH)3Catalyst is by W metal, Pt metal, metal hydroxides Ni
(OH)2And rare-earth hydroxide La (OH)3Composition, chemical formula are NiPt-Ni (OH)2/La(OH)3, wherein the content of Ni be
The content of 2.1~13.0wt.%, Pt are 8.1~54.1wt.%, Ni (OH)2Content be 0.8~5.1wt.%, La (OH)3's
Content is 27.7~88.5wt.%.
NiPt-Ni (OH) of the present invention2/La(OH)3Catalyst is made at normal temperatures and pressures using precipitating reduction method,
Specifically includes the following steps:
1) La (OH) is added in water3And it is uniformly mixed；
2) precursor solution of Ni and Pt is added into the solution that step 1) obtains, is ultrasonically treated and is uniformly mixed；
3) NaOH is added into the solution that step 2) obtains, is ultrasonically treated and is uniformly mixed；
4) NaBH is added into the solution that step 3) obtains4, it is uniformly mixed and reacts a period of time；
5) solid matter is isolated from the solution that step 4) obtains, and is washed and dry, is obtained the NiPt-Ni
(OH)2/La(OH)3Catalyst.
In above-mentioned preparation method, the precursor solution of Ni and Pt are the aqueous solution of Ni salt and Pt salt, preferably NiCl2With
K2PtCl4Aqueous solution.
In above-mentioned preparation method, the molar ratio of Ni salt and Pt salt is 1:1.
In above-mentioned preparation method, the reaction time described in step 4) is 10min.
Above-mentioned NiPt-Ni (OH)2/La(OH)3Catalyst can be used for being catalyzed hydrazine and produce hydrogen, and catalytic performance is excellent.Its
In, NiPt-Ni (OH)2/La(OH)3Catalyst is a kind of black powder substance, can be recycled from reaction system by being centrifuged,
With the features such as catalytic activity height, stability is good；Under conditions of room temperature (298K) alkali-free can efficient catalytic hydrazine produce hydrogen, turn
Change frequency (TOF) and is up to 303.2h-1, TOF value catalyst more highest than activity under the alkali-free additive reported at present is one high
The order of magnitude.If 2M NaOH is added, TOF value respectively reaches 857.1h at 298K and 303K-1And 1034.5h-1, than current
The highest catalyst of activity of report is more preferable.
The invention has the advantages that 1) preparation method is simple；2) composite nano-catalyst prepared by is in room temperature alkali-free
In the case where can efficient catalytic hydrazine produce hydrogen, transformation frequency is up to 303.2h-1, hydrogen selective 95%；3) catalyst has
There is good cyclical stability；4) catalyst is easily recycled, reusable, is had a good application prospect.
Detailed description of the invention
Fig. 1 is 1 gained NiPt-Ni (OH) of the embodiment of the present invention2/La(OH)3Catalyst and its polycrystalline X of contrast sample are penetrated
Ray diffraction diagram.
Fig. 2 is 1 gained NiPt-Ni (OH) of the embodiment of the present invention2/La(OH)3The transmission electron microscope picture of catalyst.
Fig. 3 is 1 gained NiPt-Ni (OH) of comparative example of the present invention2The Raman spectrum and infrared spectrogram of catalyst.
Fig. 4 is 1 gained NiPt-Ni (OH) of the embodiment of the present invention2/La(OH)3(left figure is the photoelectron spectroscopy figure of catalyst
Ni 2p spectrogram, right figure are Pt 4f spectrogram).
Fig. 5 is 1 gained NiPt-Ni (OH) of the embodiment of the present invention2/La(OH)3Photoelectron spectroscopy figure (the O 1s spectrum of catalyst
Figure).
Fig. 6 is 2 gained NiPt-Ni (OH) of the embodiment of the present invention 1, comparative example 1 and comparative example2/La(OH)3Catalyst,
NiPt-Ni(OH)2Catalyst and NiPt-Ni (OH)2+La(OH)3Mixture is catalyzed hydrazine decomposability test chart at room temperature.
Fig. 7 is 1 gained NiPt-Ni (OH) of the embodiment of the present invention2/La(OH)3Hydrazine decomposability is catalyzed under catalyst different temperatures
It can test chart.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1:
1) 40mg La (OH) is added in 4mL water310min is stirred by ultrasonic, obtains uniform solution；
2) solution containing 0.05mmol nickel chloride and 0.06mmol Platinous Potassium Chloride is added into the solution of step 1), surpasses
Sound stirs 10min；
3) NaOH of 36mg is added into the solution of step 2), stirs ultrasound 10min；
4) NaBH of 30mg is added into the solution of step 3)4, stirring to fully reacting；
5) by step 4) products therefrom centrifuge washing to neutrality, separation is dried to obtain NiPt-Ni (OH)2/La(OH)3Catalysis
Agent.
Comparative example 1:
By the addition 40mg La (OH) of the step 1) of embodiment 13It is changed to that 0mg La (OH) is added3.Other steps are the same as implementation
Example 1 obtains NiPt-Ni (OH)2Catalyst.
Embodiment 2:
By the addition 40mg La (OH) of the step 1) of embodiment 13It is changed to that 5mg La (OH) is added3.Other steps are the same as implementation
Example 1 obtains NiPt-Ni (OH)2/La(OH)3Catalyst.
Embodiment 3:
By the addition 40mg La (OH) of the step 1) of embodiment 13It is changed to that 100mg La (OH) is added3.Other steps are the same as real
Example 1 is applied, NiPt-Ni (OH) is obtained2/La(OH)3Catalyst.
Embodiment 4:
The NaOH of the addition 36mg of the step 3) of embodiment 1 is changed to the NaOH of 5mg is added.Other steps with embodiment 1,
Obtain NiPt-Ni (OH)2/La(OH)3Catalyst.
Embodiment 5:
The NaOH of the addition 36mg of the step 3) of embodiment 1 is changed to the NaOH of 50mg is added.The same embodiment of other steps
1, obtain NiPt-Ni (OH)2/La(OH)3Catalyst.
Embodiment 6:
By the NaBH of the addition 30mg of the step 4) of embodiment 14It is changed to that the NaBH of 15mg is added4.The same embodiment of other steps
1, obtain NiPt-Ni (OH)2/La(OH)3Catalyst.
Embodiment 7:
By the NaBH of the addition 30mg of the step 4) of embodiment 14It is changed to that the NaBH of 100mg is added4.Other steps are the same as implementation
Example 1 obtains NiPt-Ni (OH)2/La(OH)3Catalyst.
Comparative example 2:
The step of embodiment 1, is changed to 0mg La (OH) is added3.Other steps obtain NiPt-Ni (OH) with embodiment 12
Catalyst, and step 6) is added: by gained NiPt-Ni (OH)2Catalyst and 40mg La (OH)3It stirs evenly, obtains NiPt-
Ni(OH)2+La(OH)3Mixture.
Embodiment 9-11
It is (right respectively for hydrazine decomposing hydrogen-production using embodiment 1, comparative example 1 and the resulting composite nano-catalyst of comparative example 2
Embodiment 9,10 and 11) is answered, catalyst is placed in the 50mL three-necked flask of the ultrapure water containing 4mL, hydrazine hydrate is then added.In
(result is as shown in Figure 6) is reacted under 298K, after following result (table one):
Table one
Embodiment 12-16:
Using 1 resulting NiPt-Ni (OH) of embodiment2/La(OH)3Catalyst is catalyzed under five different reaction temperatures
Hydrazine decomposing hydrogen-production (respectively corresponds embodiment 12-16).Catalyst is placed in the three-necked flask of the ultrapure water containing 5mL, is then added
Hydrazine hydrate.Reacted (result is as shown in Figure 7) at different temperatures, after following result (table two)
Table two
Claims (9)
1. a kind of NiPt-Ni (OH)2/La(OH)3Catalyst, by W metal, Pt metal, metal hydroxides Ni (OH)2And it is dilute
Native hydroxide La (OH)3Composition, chemical formula are NiPt-Ni (OH)2/La(OH)3, wherein the content of Ni is 2~15wt.%,
The content of Pt is 8~55wt.%, Ni (OH)2Content be 0.5~6wt.%, La (OH)3Content be 27~89wt.%.
2. NiPt-Ni (OH) according to claim 12/La(OH)3Catalyst, it is characterised in that: the content of Ni be 2.1~
The content of 13.0wt.%, Pt are 8.1~54.1wt.%, Ni (OH)2Content be 0.8~5.1wt.%, La (OH)3Content
For 27.7~88.5wt.%.
3. a kind of NiPt-Ni (OH)2/La(OH)3The preparation method of catalyst, specifically includes the following steps:
1) La (OH) is added in water3And it is uniformly mixed；
2) precursor solution of Ni and Pt is added into the solution that step 1) obtains, is ultrasonically treated and is uniformly mixed；
3) NaOH is added into the solution that step 2) obtains, is ultrasonically treated and is uniformly mixed；
4) NaBH is added into the solution that step 3) obtains4, it is uniformly mixed and reacts a period of time；
5) solid matter is isolated from the solution that step 4) obtains, and is washed and dry, is obtained the NiPt-Ni (OH)2/La
(OH)3Catalyst.
4. according to the method described in claim 3, it is characterized by: the precursor solution of Ni and Pt is the water-soluble of Ni salt and Pt salt
Liquid.
5. according to the method described in claim 4, it is characterized by: the precursor solution of Ni and Pt is NiCl2And K2PtCl4's
Aqueous solution.
6. according to the method described in claim 4, it is characterized by: the molar ratio of Ni salt and Pt salt is 1:1.
7. according to the method described in claim 3, it is characterized by: the reaction time described in step 4) is 10min.
8. NiPt-Ni (OH) according to claim 1 or 22/La(OH)3The application of catalyst.
9. application according to claim 8, it is characterised in that: the NiPt-Ni (OH)2/La(OH)3Catalyst is used for
It is catalyzed hydrazine and produces hydrogen.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113713839A (en) * | 2020-05-25 | 2021-11-30 | 中国科学院大连化学物理研究所 | Boron nitride loaded metal ruthenium catalyst, preparation method and application in imine preparation |
| CN115445665A (en) * | 2022-08-29 | 2022-12-09 | 江西师范大学 | Composite nano catalyst for decomposing hydrazine hydrate to produce hydrogen and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113713839A (en) * | 2020-05-25 | 2021-11-30 | 中国科学院大连化学物理研究所 | Boron nitride loaded metal ruthenium catalyst, preparation method and application in imine preparation |
| CN113713839B (en) * | 2020-05-25 | 2023-04-07 | 中国科学院大连化学物理研究所 | Boron nitride loaded metal ruthenium catalyst, preparation method and application in imine preparation |
| CN115445665A (en) * | 2022-08-29 | 2022-12-09 | 江西师范大学 | Composite nano catalyst for decomposing hydrazine hydrate to produce hydrogen and preparation method and application thereof |
| CN115445665B (en) * | 2022-08-29 | 2023-10-13 | 江西师范大学 | Composite nano catalyst for decomposing hydrazine hydrate to produce hydrogen and preparation method and application thereof |
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